反応 #2021478

反応方程式

sodium acetate

2-(N-ethylanilino)ethyl acetate

phosphoryl chloride

→

2-(ethyl(4-formylphenyl)amino)ethyl acetate

収率 84.2%

溶媒

dimethylformamide

dimethylformamide

反応条件

後処理

1. 1
   その他to react for 6 hours at room temperature
2. 2
   抽出An organic layer was extracted with ethyl acetate

実験手順

After adding 55.8 g of ice-cooled phosphoryl chloride to 26.6 g of dimethylformamide, a solution of 63.0 g of the 2-(N-ethylanilino)ethyl acetate in 40 ml of dimethylformamide was slowly added at room temperature, this was caused to react for 6 hours at room temperature while stirring, and then poured into an aqueous solution of 150 g of sodium acetate under ice cooling. An organic layer was extracted with ethyl acetate and the solvent was boiled off under reduced pressure. This was refined by silica gel column chromatography to yield 60.2 g of 2-(ethyl(4-formylphenyl)amino)ethyl acetate.

出典